CA2317692A1 - Pyrogenically produced aluminium oxide - Google Patents

Pyrogenically produced aluminium oxide Download PDF

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Publication number
CA2317692A1
CA2317692A1 CA002317692A CA2317692A CA2317692A1 CA 2317692 A1 CA2317692 A1 CA 2317692A1 CA 002317692 A CA002317692 A CA 002317692A CA 2317692 A CA2317692 A CA 2317692A CA 2317692 A1 CA2317692 A1 CA 2317692A1
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CA
Canada
Prior art keywords
good
aluminium oxide
surface area
industry
pyrogenically produced
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Abandoned
Application number
CA002317692A
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French (fr)
Inventor
Peer Plambeck-Fischer
Volker Hamm
Thomas Scharfe
Helmut Mangold
Thomas Hennig
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Evonik Operations GmbH
Original Assignee
Degussa Huels AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Degussa Huels AG filed Critical Degussa Huels AG
Publication of CA2317692A1 publication Critical patent/CA2317692A1/en
Abandoned legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/02Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/30Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
    • C01F7/302Hydrolysis or oxidation of gaseous aluminium compounds in the gaseous phase
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/02Aluminium oxide; Aluminium hydroxide; Aluminates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/11Powder tap density
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/12Surface area
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/90Other properties not specified above
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/25Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/25Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
    • Y10T428/256Heavy metal or aluminum or compound thereof
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/25Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
    • Y10T428/256Heavy metal or aluminum or compound thereof
    • Y10T428/257Iron oxide or aluminum oxide
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/29Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982Particulate matter [e.g., sphere, flake, etc.]

Abstract

Pyrogenically produced aluminium oxide, in which the BET
specific surface area is greater than 115 m2/g and the Sears index is over 8 ml/2g and the dibutyl phthalate absorption as a powder measured with a 16 g weighed portion is not measurable, is produced by means of flame oxidation or preferably flame hydrolysis, whereby a vaporisable aluminium compound is used as starting material.
The aluminium oxide can be used as an ink-absorbing substance in inkjet media and also as a filler, as a substrate, as a catalytically active substance, as a starting material for the production of dispersions, as a polishing material (CMP applications), as a ceramic raw material, in the electronics industry, in the cosmetics industry, as an additive in the silicone and rubber industry, to adjust the rheology of liquid systems, as a heat stabiliser, in the paint industry.

Description

Pyrogenically produced aluminium oxide The invention concerns a pyrogenically produced aluminium oxide, a method for its production and its use.
Applications in the paper industry call for readily dispersible fillers which absorb ink rapidly when used in inkjet paper or inkjet films and which help to give colours a high brilliance. The present invention concerns a specially produced aluminium oxide which, by virtue of its properties in corresponding coating slip formulations, is capable of reproducing inks applied by an inkjet printer onto these media containing this special aluminium oxide with very high brilliance and colour fidelity.
It also concerns the application of this aluminium oxide in the manufacture of ink-receiving layers such as are conventional in inkjet media (e. g. paper, films, fabric, etc.).
The invention provides a high surface area, pyrogenically produced aluminium oxide, characterised in that the BET
specific surface area is greater than 115 mz/g, and the Sears index is over 8 ml/2g.
In an embodiment of the invention, the aluminium oxide is characterised in that the dibutyl phthalate absorption by the powder measured with a 16 g weighed portion is not measurable (no end-point detection).
The pyrogenically produced aluminium oxide according to the invention can be produced by means of flame oxidation or preferably flame hydrolysis, whereby a vaporisable aluminium compound, preferably chloride, is used as starting material.
The invention also provides the use of the aluminium oxide according to the invention as an ink-absorbing substance in inkjet media.
The invention also provides the use of the high surface area aluminium oxide according to the invention as a filler, as a substrate, as a catalytically active substance, as a starting material for the production of dispersions, as a polishing material (CMP applications), as a ceramic raw material, in the electronics industry, in the cosmetics industry, as an additive in the silicone and rubber industry, to adjust the rheology of liquid systems, as a heat stabiliser, in the paint industry.
The pyrogenically produced aluminium oxide according to the invention as an ink-absorbing substance displays the following properties:
Good optical density and dot resolution, high ink absorption, rapid ink drying time, no bleeding (running together of inks), good water resistance after drying, no colour shifts, no breakdown of inks after extended periods.
In comparison to known commercially available products (Aluminiumoxid C and Aerosil MOX 170, both from Degussa-Hiils AG), the aluminium oxide according to the invention exhibits very good properties for the manufacture of inkjet receiving layers, both alone and in combination with other fillers. It is characterised by enhanced brilliance and depth of colour. These properties are of particular benefit in ink-receiving layers that are used for photographic quality reproduction. Vfleather resistance to water and light is also improved, which is advantageous for outdoor applications.
Example 1 320 kg/h of previously vaporised aluminium trichloride (A1C13) are burned together with 100 Nm3/h hydrogen and 450 Nm3/h air in a burner of a known design.
After the flame reaction the fine-particle high surface area aluminium oxide is separated in a filter or cyclone from the hydrochloric acid gases generated at the same time, whereby any HC1 traces still adhering are then removed by treatment with moist air at elevated temperature.
The high surface area pyrogenic aluminium oxide produced exhibits the physicochemical properties indicated in Table 1. Data for the commercially available pyrogenic aluminium oxide produced by Degussa-Hiils AG in Frankfurt am Main is also included in Table 1 for the purposes of comparison.
(Trade name Aluminiumoxid C).
Table 1 Unit Sigh surface area Aluminium-aluminium oxide oxid C

according to the invention Alu 130 BET m' / g 121 10 0 specific surface area Sears index ml/2g 9.38 7.05 (pH 4 to 9 ) pH 4~ aqueous 4.93 4.5 dispersion Loss on drying wt.~ 3.3 3.0 Bulk density g/1 55 4g Compacted bulk g/1 63 57 density DBP absorption wt.~ not measurable , 231 no end point can be determined.

DBP: dibutyl phthalate Measurement of the Sears index is described in EP 0 717 008.
Example 2 Manufacture of the coating slip and coating:
30 parts by weight of polyvinyl alcohol Mowiol 28-99 (Clariant), 80 parts by weight of Sipernat 310 (precipitated silicic acid, Degussa-Hiils AG) and in each case 20 parts by weight of the pyrogenically produced oxides described above are used. The solids content is adjusted to 18 ~. This aqueous dispersion is stirred for 30 min at 3000 rpm with a high-speed mixer. This coating slip is applied to a 70 g/m2 base paper by means of a profiled doctor bar. The coating slip is dried with hot air. The rate of application in the dry state is 10 g/mz.
Results Aerosil MOX 170 Aluminiumoxid Alu 130 C

Brilliance good good-very good very good Weather satisfactory good good-very good resistance Example 3 Manufacture of the coating slip:
35 parts by weight of polyvinyl alcohol Mowiol 28-99 (Clariant) and in each case 100 parts by weight of the pyrogenically produced oxides described above are used. The solids content is adjusted to 15 $. This dispersion is homogenised. This coating slip is applied to a 100 micrometer thick polyester film by means of a profiled doctor bar. The coating slip is dried with hot air. The wet film thickness is 120 micrometers.

Results Aerosil MOX 170 Alu C Alu 130 Adhesion to adequate-good good-very good film satisfactory Brilliance satisfactory good good-very good Weather satisfactory good good-very good resistance Ink absorption good- good very good satisfactory Gloss good- good-very good very good satisfactory Example 4 Manufacture of the coating slip:
5 70 parts by weight of polyvinyl alcohol Mowiol 5-88 (Clariant), 20 parts by weight of PVP/VA W-735 (polyvinyl pyrrolidone-polyvinyl acetate copolymer, ISP), 10 parts of polyvinyl pyrrolidone K-30 (ISP) and in each case 50 parts by weight of the pyrogenically produced oxides described above are used.
The solids content is adjusted to 20 ~. The coating slip is applied by means of a profiled doctor bar to a 100 micrometer thick polyester film in a wet film thickness of 80 micrometers. The coating slip is dried with hot air.
Results Aerosil MOX 170 Alu C Alu 130 Brilliance good good-ve ry good very good Weather satisfactory- good good-very good resistance good Transparency satisfactory good good-very good Gloss satisfactory- good-ve ry good very good good These results illustrate the application-related advantages of the aluminium oxide Alu 130 according to the invention.
Example 5 For the purposes of comparison, Aluminiumoxid C and MOX 170 (both Degussa-Hills AG Frankfurt) were used in addition to the high surface area aluminium oxide 130 according to the invention.
Manufacture of the coating slip and coating:
Solution A is a 10 percent (relative to PVA) aqueous solution of polyvinyl alcohol (solid, abbreviation PVA) Mowiol 28-99 from Clariant.
Distilled water is added to this solution to form a solution B. Sipernat 310 (precipitated silicic acid, Degussa-Hills AG) and each of the pyrogenically produced oxides are added to this solution B to form the coating slip C. This coating slip exhibits a mass ratio of 80 parts Sipernat 310 to 20 parts pyrogenic oxide to 30 parts PVA, relative to the solids. The total solids content is 18 The coating slip C is dispersed for 30 minutes at 3000 rpm in a high-speed mixer. The coating slip is then applied to a 70 g/m2 base paper by means of a profiled doctor bar and dried with hot air. The rate of application in the dry state is 10 g/ma.
The printing tests are performed on an Epson Stylus Colour 800 at maximum resolution (1440 * 720 dpi).
Results Aerosil MOX 170 Alu C high surface area aluminium oxide according to the invention Colour good good-very very good intensity good Colour satisfactory good good-very good stability Example 6 Coating slip formulation For the purposes of comparison, Aluminiumoxid C and MOX 170 (both Degussa-Hills AG Frankfurt) are used as additional oxides in addition to the high surface area aluminium oxide 130 according to the invention.
An aqueous dispersion is produced from these three different pyrogenic oxides using a rotor-stator system (Ultra-Turrax) for a dispersion period of 30 minutes in a double-walled vessel (with water cooling). A 25 percent dispersion (relative to the solid) (w = 0.25) is produced containing a proportion by weight of 0.5 ~ acetic acid.
Manufacture of the coating slip:
Solution A is an 8 percent (relative to PVA) aqueous solution of polyvinyl alcohol (solid, abbreviation PVA) Mowiol 40-88 from Clariant.
This solution A is diluted with distilled water to produce a solution B. Each of the various metal oxide dispersions is added to solution B to form a coating slip C. The coating slip C exhibits a mass ratio of 100 parts pyrogenic oxide to 25 parts PVA, relative to the solid. The total solids content is 15 ~. This coating slip is applied by means of a profiled doctor bar to a 100 micrometer thick polyester film and dried with hot air. The wet film thickness is 120 micrometers.
It was not possible to manufacture an adhesive coating using Aerosil MOX 170.
For this mixed oxide the proportion had to be increased to a ratio of 100 parts Aerosil to 40 parts PVA, relative to the solids ratio.
Results Aerosil MOX 170 Alu C High surface area aluminium oxide according to the invention Adhesion to adequate good good-very good film Brilliance satisfactory good-ver y good very good Colour satisfactory good-ve ry good very good stability Ink very good good good-very good absorption Gloss poor good-very good very good Example 7 Coating slip formulation For the purposes of comparison, Aluminiumoxid C and MOX 170 (both Degussa-Hills AG Frankfurt) were used as additional oxides in addition to the high surface area aluminium oxide 130 according to the invention.
Solution A is a 20 percent (relative to PVA) aqueous solution of polyvinyl alcohol (solid, abbreviation PVA) 4-88 from Clariant.
Solution B is a 50 percent (relative to the copolymer) aqueous solution of a copolymer of vinyl pyrrolidone and vinyl acetate (abbreviation PVP / VA) W 735 from ISP.

Solution C is a 20 percent (relative to PVP) aqueous solution of polyvinyl pyrrolidone (abbreviation PVP) K - 30 from ISP.
These three solutions are mixed in the above sequence and 5 in the following ratio (70 parts by weight PVA . 20 parts PVP / VA . 10 parts PVP, relative to the solid) and diluted with water so that a coating slip with a total solids content of 20 ~ is obtained by addition of 50 parts of each of the metal oxides. This dispersion is dispersed for 30 10 minutes at 10000 rpm in a suitable dispersion device such as an Ultra-Turrax from Janke & Kunkel with a rotor-stator system. The coating slip is applied by means of a profiled doctor bar to a 100 micrometer thick polyester film in a wet film thickness of 80 micrometers and dried with hot air.
Results Aerosil MOX Alu C high surface area 170 aluminium oxide according to the invention Brilliance good good-ve ry very good good Colour satisfactory good good-very good stability -good Transparency satisfactory good good-very good Gloss satisfactory good-ve ry very good -good good . 990148 FA / AL
Advantages:
In comparison to the commercially available products (Aluminiumoxid C and Aerosil MOX 170, both Degussa-Huls AG) the aluminium oxide according to the invention exhibits very good properties in the manufacture of inkjet receiving layers both alone and in combination with other fillers. It is characterised by enhanced brilliance and depth of colour. These properties are of particular benefit in ink-receiving layers that are used for photographic quality reproduction. It also demonstrates improved colour stability in the presence of water and light, which is advantageous for outdoor applications.

Claims (5)

1. High surface area pyrogenically produced aluminium oxide, characterised in that the BET specific surface area is greater than 115 m2/g and the Sears index is over 8 ml/2g.
2. Pyrogenically produced aluminium oxide according to claim 1, characterised in that the dibutyl phthalate absorption of the powder measured with a 16 g weighed portion is not measurable (no end-point detection).
3. Pyrogenically produced aluminium oxide according to claims 1 and 2, characterised in that it is produced by means of flame oxidation or preferably flame hydrolysis, whereby a vaporisable aluminium compound, preferably chloride, is used as starting material.
4.Use of the high surface area aluminium oxide according to claim 1 as an ink-absorbing substance in inkjet media.
5. Use of the high surface area aluminium oxide according to claim 1 as a filler, as a substrate, as a catalytically active substance, as a starting material for the production of dispersions, as a polishing.
material (CMP applications), as a ceramic raw material, in the electronics industry, in the cosmetics industry, as an additive in the silicone and rubber industry, to adjust the rheology of liquid systems, as a heat stabiliser, in the paint industry.
CA002317692A 1999-09-10 2000-09-07 Pyrogenically produced aluminium oxide Abandoned CA2317692A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19943291.0 1999-09-10
DE19943291A DE19943291A1 (en) 1999-09-10 1999-09-10 Pyrogenic alumina

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CA2317692A1 true CA2317692A1 (en) 2001-03-10

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US (1) US6680109B1 (en)
EP (1) EP1083151B1 (en)
JP (1) JP3529712B2 (en)
CN (1) CN1287974A (en)
AT (1) ATE212320T1 (en)
BR (1) BR0004058A (en)
CA (1) CA2317692A1 (en)
DE (2) DE19943291A1 (en)
DK (1) DK1083151T3 (en)
ES (1) ES2170743T3 (en)
IL (1) IL138315A0 (en)
NO (1) NO321445B1 (en)
PL (1) PL342441A1 (en)
TW (1) TWI232205B (en)

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US8241594B2 (en) 2007-05-21 2012-08-14 Orbite Aluminae Inc. Processes for extracting aluminum and iron from aluminous ores
US9023301B2 (en) 2012-01-10 2015-05-05 Orbite Aluminae Inc. Processes for treating red mud
US9150428B2 (en) 2011-06-03 2015-10-06 Orbite Aluminae Inc. Methods for separating iron ions from aluminum ions
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US9382600B2 (en) 2011-09-16 2016-07-05 Orbite Technologies Inc. Processes for preparing alumina and various other products
US9410227B2 (en) 2011-05-04 2016-08-09 Orbite Technologies Inc. Processes for recovering rare earth elements from various ores
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Cited By (17)

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Publication number Priority date Publication date Assignee Title
US7572854B2 (en) 2001-10-25 2009-08-11 Degussa Ag Dispersion of aluminium oxide
US7985792B2 (en) 2001-10-25 2011-07-26 Evonik Degussa Gmbh Dispersion of aluminium oxide
US8241594B2 (en) 2007-05-21 2012-08-14 Orbite Aluminae Inc. Processes for extracting aluminum and iron from aluminous ores
US8337789B2 (en) 2007-05-21 2012-12-25 Orsite Aluminae Inc. Processes for extracting aluminum from aluminous ores
US8597600B2 (en) 2007-05-21 2013-12-03 Orbite Aluminae Inc. Processes for extracting aluminum from aluminous ores
US9260767B2 (en) 2011-03-18 2016-02-16 Orbite Technologies Inc. Processes for recovering rare earth elements from aluminum-bearing materials
US9945009B2 (en) 2011-03-18 2018-04-17 Orbite Technologies Inc. Processes for recovering rare earth elements from aluminum-bearing materials
US9410227B2 (en) 2011-05-04 2016-08-09 Orbite Technologies Inc. Processes for recovering rare earth elements from various ores
US9150428B2 (en) 2011-06-03 2015-10-06 Orbite Aluminae Inc. Methods for separating iron ions from aluminum ions
US9382600B2 (en) 2011-09-16 2016-07-05 Orbite Technologies Inc. Processes for preparing alumina and various other products
US10174402B2 (en) 2011-09-16 2019-01-08 Orbite Technologies Inc. Processes for preparing alumina and various other products
US9023301B2 (en) 2012-01-10 2015-05-05 Orbite Aluminae Inc. Processes for treating red mud
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ATE212320T1 (en) 2002-02-15
ES2170743T3 (en) 2002-08-16
EP1083151A1 (en) 2001-03-14
IL138315A0 (en) 2001-10-31
JP2001146419A (en) 2001-05-29
JP3529712B2 (en) 2004-05-24
NO20004483L (en) 2001-03-12
CN1287974A (en) 2001-03-21
DK1083151T3 (en) 2002-05-06
NO20004483D0 (en) 2000-09-08
NO321445B1 (en) 2006-05-08
US6680109B1 (en) 2004-01-20

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